KR950002643B1 - Mno2 coating firing method - Google Patents
Mno2 coating firing method Download PDFInfo
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- KR950002643B1 KR950002643B1 KR1019920013584A KR920013584A KR950002643B1 KR 950002643 B1 KR950002643 B1 KR 950002643B1 KR 1019920013584 A KR1019920013584 A KR 1019920013584A KR 920013584 A KR920013584 A KR 920013584A KR 950002643 B1 KR950002643 B1 KR 950002643B1
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- South Korea
- Prior art keywords
- tantalum
- manganese dioxide
- mno
- mno2
- manganese
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- 239000011248 coating agent Substances 0.000 title claims description 7
- 238000000576 coating method Methods 0.000 title claims description 7
- 238000000034 method Methods 0.000 title abstract description 28
- 238000010304 firing Methods 0.000 title description 9
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 64
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003990 capacitor Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 21
- 229910052715 tantalum Inorganic materials 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000011572 manganese Substances 0.000 claims description 9
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 9
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
Description
제1도는 (a)(b)(c)(d)는 종래의 탄탈 전해콘덴서의 소성 방법을 도시하는 도면.1 (a), (b), (c), and (d) show a firing method of a conventional tantalum electrolytic capacitor.
제2도의 (a)(b)(c)(d)(e)는 본 발명의 탄탈 전해콘덴서의 소성 방법을 도시하는 도면.(A) (b) (c) (d) (e) of FIG. 2 is a figure which shows the baking method of the tantalum electrolytic capacitor of this invention.
본 발명은 탄탈 전해콘덴서의 소성 방법에 관한 것으로, 특히 전해질 형성시 열분해 방식에 따른 단점을 개선하고자 이산화망간 분말을 디핑방식으로 코딩한 탄탈 전해콘덴서의 소성 방법에 관한 것이다.The present invention relates to a firing method of a tantalum electrolytic capacitor, and more particularly, to a firing method of a tantalum electrolytic capacitor in which a manganese dioxide powder is coded by a dipping method in order to improve the disadvantage of the pyrolysis method when forming an electrolyte.
일반적으로, 탄탈 콘덴서의 제조방법은 탄탈분말에 바인더를 혼합하여 펠릿을 성형하는 성형공정, 바인더와 불순물을 제거하고 순수 탄탈분말을 소결시키는 소결공정, 상술한 펠릿을 알루미늄 벨트에 용정하는 펠릿용접공정, 필릿표면에 인산수용액에서 전기분해시켜 유전체(Ta2O5)를 형성하는 화성 공정이 순차적으로 진행되어 소성로에서 이산화망간 고체 전해질층(MnO2)을 형성하는 소성공정으로 이어지며 이후, 조립, 리드용접, 외장공정등으로 진행된다.In general, a method of manufacturing a tantalum capacitor includes a molding process of forming pellets by mixing a binder with tantalum powder, a sintering process of removing binder and impurities and sintering pure tantalum powder, and a pellet welding process of melting the above-mentioned pellets on an aluminum belt. The chemical conversion process is performed to form dielectric (Ta 2 O 5 ) by electrolysis in aqueous solution of phosphate on fillet surface, followed by the sintering process to form manganese dioxide solid electrolyte layer (MnO 2 ) in the kiln. Proceed with welding, exterior process, etc.
상기 소성공정에서는 통상적으로 소자의 기공내부에 있는 산화피막의 표면에 이산화망간층(Mn02)을 증착시키기 위하여 질산망간(Mn(NO3)2)의 수용액중에 소자를 침적하여 함침시킨후 가열 분해하여 이산화망간층(MnO2)을 얻는다.In the firing process, in order to deposit a manganese dioxide layer (Mn0 2 ) on the surface of the oxide film in the pores of the device, the element is immersed in an aqueous solution of manganese nitrate (Mn (NO 3 ) 2 ) and then thermally decomposed Manganese dioxide layer (MnO 2 ) is obtained.
따라서 제1도는 종래의 탄탈 전해콘덴서의 소성방법에서 질산망간의 열분해 공정을 나타낸 것으로, (a)도에서는 소자 탄탈금속(Ta)을 전기분해에 의하여 유전체(Ta2O5)피막을 형성한 후 2차인 (b)도에서는 탄탈소자를 질산망간(Mn(NO3)2) 수용액에 소자를 함침시켜 산화탄탈피막(Ta2O5) 위해 8-13회의 반복 도포한후 3차인 (c)도에서는 전기로 내에 소자를 넣고 온도(240℃-300℃)로 가열하여 열분해하면 즉, Mn(NO3)2----→ MnO2+2NO2↑에 의해 산화탄탈피막(Ta2O5)위에 이산화망간이 형성되며, (d)도에서는 종래의 전해질이 형성된 완성품을 도시한다.Therefore, FIG. 1 shows a pyrolysis process of manganese nitrate in the conventional firing method of a tantalum electrolytic capacitor, and in (a), after forming a dielectric (Ta 2 O 5 ) film by electrolysis of element tantalum metal (Ta) In the second phosphorus (b), the tantalum element is impregnated with an aqueous solution of manganese nitrate (Mn (NO 3 ) 2 ) and repeatedly applied 8-13 times to the tantalum oxide coating (Ta 2 O 5 ). In the electric furnace, the element is placed in an electric furnace and heated to a temperature (240 ° C.-300 ° C.) to pyrolyze, that is, tantalum oxide film (Ta 2 O 5 ) by Mn (NO 3 ) 2 ---- → MnO 2 + 2NO 2 ↑. Manganese dioxide is formed thereon, and (d) shows a finished product in which a conventional electrolyte is formed.
그러나, 종래의 소성공정에서 산화탄탈피막(Ta2O5)위에 이산화망간층을 형성하기 위해서 질산망간 수용액(Mn(NO3)2)에 소결소자를 함침하면 얇게 도포되기 때문에 8-13회를 반복해야 하고, 도포한 후에는 고온(240℃-300℃)의 전기로에서 가열하여 열분해하는 공정을 거쳐야 한다. 이는 8∼13회를 반복함으로써 작업공수 및 공정시간이 늘어나 아울러 문제점을 초래함과 고온의 전기로에서 장시간에 걸쳐서 열분해 함으로써 열적 스트레스를 초래하여 산화탄탈피막의 손상을 가져와서 누설전류가 증가되는 문제점이 발생하게 하였다.However, in order to form a manganese dioxide layer on the tantalum oxide coating (Ta 2 O 5 ) in the conventional firing process, the sintered element is impregnated in an aqueous solution of manganese nitrate (Mn (NO 3 ) 2 ), and thus 8 to 13 times is repeated. After application, the process must be pyrolyzed by heating in an electric furnace of high temperature (240 ° C-300 ° C). This is repeated 8 to 13 times to increase the labor and process time, and also cause problems, and thermal decomposition by thermal decomposition for a long time in a high-temperature electric furnace, causing damage to the tantalum oxide film, which increases the leakage current Generated.
본 발명은 종래의 문제점을 해결하기 위해 제안된 것으로, 질산망간 수용액에 8∼13회 함침시켜 열분해하는 공정을 질산망간 수용액에 3-4회 도포하여 열분해하는 공정으로 단순화시킨 후에 직접 이산화망간액(MnO2)을 디핑방식으로 다량 코팅하여 저온(약100℃)에서 건조시킴으로서 동일한 이산화망간층 형성효과를 달성하면서도 함침 횟수 반복에 따른 작업공수와 공정시간 절감을 실현하며 또한 장시간의 열적 스트레스(Stres)에 의한 누설전류의 감소를 실현시키는 것이 목적이다.The present invention has been proposed in order to solve the conventional problems, and it is directly manganese dioxide liquid (MnO) after simplifying the process of pyrolysis by impregnating 8 to 13 times in aqueous solution of manganese nitrate 3-4 times in the solution of manganese nitrate 2 ) By coating a large amount by dipping method and drying at low temperature (about 100 ℃), it achieves the same effect of forming manganese dioxide layer, while realizing work maneuver and process time by repeated impregnation, and by long time thermal stress The purpose is to realize a reduction in the leakage current.
상술한 목적을 달성하기 위하여, 본 발명은 탄탈소자 위에 산화탄탈피막(Ta2O5)이 형성된 후 탄탈 고체 전해콘덴서의 소정공정에 있어서, 질산망간(Mn(No3)2) 수용액에 3-4회에 걸쳐 반복 함침하여 이산화망간층(MnO2)을 산화피막(Ta2O5)위에 도포하는 제1단계 ; 산화피막(Ta2O5)위에 전기로내에서 240℃-300℃온도로 가열하여 이산화망간층(MnO2)을 형성시키는 제2단계 ; 및 이산화망간 분산액(MnO2+H2O)에 상기의 소자를 도포한후 추출하여 전기로에서 100℃ 온도로 건조시켜 완성시키는 제3단계로 이루어지는 것을 특징으로 한다.In order to achieve the above object, the present invention is a tantalum oxide film (Ta 2 O 5 ) is formed on the tantalum element, and then in a predetermined process of the tantalum solid electrolytic capacitor, manganese nitrate (Mn (No 3 ) 2 ) aqueous solution 3- Repeatedly impregnating four times to apply a manganese dioxide layer (MnO 2 ) onto the oxide film (Ta 2 O 5 ); A second step of forming a manganese dioxide layer (MnO 2 ) by heating to 240 ° C.-300 ° C. in an electric furnace on the oxide film Ta 2 O 5 ; And a third step of coating the device on a manganese dioxide dispersion (MnO 2 + H 2 O), extracting the same, and drying the same to 100 ° C. in an electric furnace.
이하에서는 참부도면을 참조하여 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail with reference to the true drawing.
제2도는 탄탈 전해콘덴서의 소성방법을 도시하는 도면으로써 화성공정에서 탄탈소자 표면에 산화탄탈피막(Ta2O5)이 증착된 후 그의 표면에 전해질의 이산화망간층(MnO2)을 형성하는 공정이 소성공정이다.2 is a diagram illustrating a firing method of a tantalum electrolytic capacitor, in which a process of forming a tantalum oxide film (Ta 2 O 5 ) on the surface of a tantalum element in a chemical conversion process and then forming a manganese dioxide layer (MnO 2 ) of an electrolyte on the surface thereof. Firing process.
즉, 탄탈소자 몸체에서 산화탈탈피막(Ta2O5)이 형성된 상태에서 질산망간(Mn(No3)2) 수용액에 3-4회에 걸쳐 소자를 반복 함침시켜 묻힌 후 질산망간층(Mn(NO3)2)을 전기로 내에서 240℃-300℃로 열분해(Mn(NO3)2----＞ MnO2+2NO2↑ )시켜 이산화망간(MnO2)을 탄탈소자 몸체의 산화피막(Ta2O5)위에 도포를 완료시킨다. 이어서, 이산화망간(MnO2) 분말과 물(H2O)이 교반된 이산화망간 분산액에 소자를 1-2회 함침시킨다.That is, in the state where the tantalum oxide stripping film (Ta 2 O 5 ) is formed in the tantalum element body, the manganese nitrate (Mn (No 3 ) 2 ) solution is repeatedly impregnated with the element three to four times, and then the manganese nitrate layer (Mn ( NO 3 ) 2 ) was pyrolyzed in an electric furnace at 240 ° C.-300 ° C. (Mn (NO 3 ) 2 ----> MnO 2 + 2NO 2 ↑) to convert manganese dioxide (MnO 2 ) into the oxide film of the tantalum element body ( Complete the application on Ta 2 O 5 ). Subsequently, the device is impregnated 1-2 times with a manganese dioxide dispersion in which manganese dioxide (MnO 2 ) powder and water (H 2 O) are stirred.
이때, 이산화망간 분산액(MnO2+H2O)의 부유성을 위해 3% 미만의 수산화암모늄(NH4OH)을 첨가하고, 소자 함침전에 이산화망간 분산액(MnO4+H2O)을 회전시켜 이산화망간(MnO2) 농도를 균일하게 함으로서 이산화망간 분산액이 도포된 소자를 전기로에서 100℃의 온도를 가해 물(H2O)을 증발시켜 탄탈소자 몸체의 산화탄탈피막(Ta2O5)위에 이산화망간(MnO2)을 증착시킨다.At this time, less than 3% of ammonium hydroxide (NH 4 OH) is added to float the manganese dioxide dispersion (MnO 2 + H 2 O), and the manganese dioxide dispersion (MnO 4 + H 2 O) is rotated before the device impregnation to manganese dioxide ( By uniformizing the concentration of MnO 2 ), the device coated with manganese dioxide dispersion was applied to a temperature of 100 ° C. in an electric furnace to evaporate water (H 2 O), and the manganese dioxide (MnO 2 ) on the tantalum oxide film (Ta 2 O 5 ) of the tantalum element body. ) Is deposited.
이에 의해 이산화망간 분산액을 이용하여 낮은 온도(100℃)의 전기로에서도 층형성이 가능해진다. 추가로, 탄탈콘덴서의 종류에 따라서 이산화망간 분산액(MnO2+H2O)의 농도를 조절하여 증착되는 이산화망간층의 두께조절이 가능하다.This enables layer formation even in an electric furnace of low temperature (100 ° C.) using a manganese dioxide dispersion. In addition, it is possible to control the thickness of the manganese dioxide layer deposited by adjusting the concentration of the manganese dioxide dispersion (MnO 2 + H 2 O) according to the type of tantalum capacitor.
전술한 구성과 작용의 본 발명에 따르면, 질산망간 수용액에 8-13회에 함침시킨 후 장시간 고온에서 열분해시키는 대신에 질산망간 수용액에 3-4회 함침시킨 후 단시간 열분해한 후 직접 이산화망간액에 다시 함침시켜 저온에서 건조시킴에 의해서 질산망간 수용액에 여러번 함침함에 따른 작업공수와 공정시간을 절감시켜주며 또한 두꺼운 질산망간을 열분해함에 의해 산화피막이 파손됨에 따라 누설전류의 발생을 방지할수 있게 해준다.According to the present invention of the above-described configuration and action, instead of impregnating the manganese nitrate aqueous solution 8-13 times and then pyrolyzing at high temperature for a long time, 3-4 times impregnation in the manganese nitrate aqueous solution and then directly decomposed directly in the manganese dioxide solution By impregnating and drying at low temperature, it saves labor time and processing time by impregnating manganese nitrate solution several times and also prevents leakage current as the oxide film is broken by thermal decomposition of thick manganese nitrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019920013584A KR950002643B1 (en) | 1992-07-29 | 1992-07-29 | Mno2 coating firing method |
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| KR1019920013584A KR950002643B1 (en) | 1992-07-29 | 1992-07-29 | Mno2 coating firing method |
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| KR940002883A KR940002883A (en) | 1994-02-19 |
| KR950002643B1 true KR950002643B1 (en) | 1995-03-23 |
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